title: Use of diffusion-ordered NMR spectroscopy and HPLC-UV-SPE-NMR to identify undeclared synthetic drugs in medicines illegally sold as phytotherapies.
abstract: The informal (and/or illegal) e-commerce of pharmaceutical formulations causes problems that governmental health agencies find hard to control, one of which concerns formulas sold as natural products. The purpose of this work was to explore the advantages and limitations of DOSY and HPLC-UV-SPE-NMR. These techniques were used to identify the components of a formula illegally marketed in Brazil as an herbal medicine possessing anti-inflammatory and analgesic properties. DOSY was able to detect the major components present at higher concentrations. Complete characterization was achieved using HPLC-UV-SPE-NMR, and 1D and 2D NMR analyses enabled the identification of known synthetic drugs. These were ranitidine and a mixture of orphenadrine citrate, piroxicam, and dexamethasone, which are co-formulated in a remedy called Rheumazim that is used to relieve severe pain, but it is prohibited in Brazil because of a lack of sufficient pharmacokinetic and pharmacodynamic information.
authors.affiliation: Departamento de Química, Universidade Federal de São Carlos, Rodovia Washington Luís, Km 235, PO Box 676, 13565-905, São Carlos, SP, Brazil.
authors.forename: Lorena M A
authors.initials: LM
authors.lastname: Silva
authors.forename: Elenilson G A
authors.initials: EG
authors.lastname: Filho
authors.forename: Sérgio S
authors.initials: SS
authors.lastname: Thomasi
authors.forename: Bianca F
authors.initials: BF
authors.lastname: Silva
authors.forename: Antonio G
authors.initials: AG
authors.lastname: Ferreira
authors.forename: Tiago
authors.initials: T
authors.lastname: Venâncio
mesh_terms: D000700:Analgesics / Q000032:analysis* / Q000138:chemical synthesis; D000894:Anti-Inflammatory Agents, Non-Steroidal / Q000032:analysis* / Q000138:chemical synthesis; D001688:Biological Products / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation; D004058:Diffusion; D004348:Drug Labeling; D009682:Magnetic Resonance Spectroscopy / Q000295:instrumentation; D015394:Molecular Structure; D028321:Plant Preparations / Q000032:analysis*; D052616:Solid Phase Extraction / Q000295:instrumentation; D013056:Spectrophotometry, Ultraviolet / Q000295:instrumentation
chemical_list: D000700:Analgesics; D000894:Anti-Inflammatory Agents, Non-Steroidal; D001688:Biological Products; D028321:Plant Preparations
keywords: DOSY; HPLC-UV-SPE-NMR; drug adulteration; illegal e-commerce; unknown formulas